CN102643195B - Production method of n-butyl acetate - Google Patents
Production method of n-butyl acetate Download PDFInfo
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- CN102643195B CN102643195B CN201210118033.7A CN201210118033A CN102643195B CN 102643195 B CN102643195 B CN 102643195B CN 201210118033 A CN201210118033 A CN 201210118033A CN 102643195 B CN102643195 B CN 102643195B
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Abstract
The invention relates to a production method of n-butyl acetate, belonging to synthesis of acetates of unitary hydroxyl compounds. The production method comprises an esterification distillation operating system, a dehydration refinement operating system and a recycling distillation operating system. The invention is characterized in that heat carried by tower top distillate gas of a dehydration refinement tower (8) is used as a heat source of a recovery tower reboiler (17); the tower top distillate gas firstly enters among tubes of the recovery tower reboiler (17), exchanges heat with the material in the tubes to get cooled, is further cooled and condensed through a dehydration refinement tower condenser A (10), and enters a phase splitter for phase splitting; and the organic phase material is totally sent into the top of the dehydration refinement tower (8) and totally refluxed. The method has the advantages of equipment investment saving, lower production cost, lower energy consumption and water resource saving. The steam consumption in the dehydration rectification process is lowered by 10%, 0.2 ton of steam can be saved per ton of products, and 100 cubic meters of tower top condensation water is saved every hour.
Description
Technical field
The present invention is a kind of production method of n-butyl acetate.Belong to acetic ester synthetic of monohydroxyl compound.
Background technology
Produce in n-butyl acetate technique in esterification process, after acetic acid and propyl carbinol react in esterifying kettle, generate n-butyl acetate, through the preliminary rectifying of esterification column, again after phase splitter phase-splitting, organic phase is sent to dehydration treating tower system, through dehydration, dealcoholysis, obtains finished product n-butyl acetate; Water, by recovery tower system, reclaims propyl carbinol and n-butyl acetate wherein, is sent to esterification column system, recycles.In dehydration treating tower system and recovery tower system, energy consumption is higher, in the positive butyl ester production cost of industrial acetic, occupies compared with large portion, has also wasted the valuable energy and the water resources of part.
Summary of the invention
The object of the invention is to avoid above-mentioned weak point of the prior art, and provide, a kind of facility investment economizes, production cost is lower, reduces energy consumption, the production method of the n-butyl acetate of saving water resource.
Object of the present invention can reach by following measure:
The production method of n-butyl acetate of the present invention, comprise esterification distillation procedure system, dehydration purification operations system and reclaim distillation procedure system, it is characterized in that utilizing dehydration treating tower 8 tower tops to distillate heat that gas the carries thermal source as recovery tower reboiler 17, described tower top distillates gas and first enters between recovery tower reboiler 17 pipes, with material-heat-exchanging in pipe, self obtain cooling simultaneously, again through dehydration treating tower condenser A10 further after cooling, condensation, enter phase splitter phase-splitting, organic phase material is all admitted to dehydration treating tower 8 tops, total reflux.
Method utilization of the present invention dehydration treating tower 8 tower tops distillate heat that gas the carries thermal source as recovery tower reboiler 17, reduce the steam consumption in production process, cooling water amount; Reduce condensing equipment investment; Save valuable water resources; Effectively realize energy-saving and cost-reducing.Compare with existing technical process, the steam consumption in same scale n-butyl acetate production equipment dehydration rectifying reduces 10%, and ton product can steam saving 0.2 ton, 100 meters of overhead condensation water saving per hour
3.
Object of the present invention can also reach by following measure:
The production method of n-butyl acetate of the present invention, working pressure >=the 0.3MPa of described dehydration purification operations system, described utilization dehydration treating tower 8 tower tops distillate heat that gas the carries thermal source as recovery tower reboiler 17, to substitute the needed heating steam of recovery tower reboiler 17 completely, need not other supplemental heat source.Because the raising of working pressure can effectively improve dehydration treating tower, 8 tower tops distillate the temperature of gas and the heat exchange efficiency of recovery tower reboiler 17 storerooms.It is preferred technical scheme.
The production method of n-butyl acetate of the present invention, dehydration treating tower 8 tower tops distillate gas and enter between recovery tower reboiler 17 pipes, after material-heat-exchanging in pipe, enter again supplementary heat exchanger 25, with the charging heat exchange of dehydration treating tower 8, the liquid that condensation is got off enters dehydration treating tower condenser A 10, then enters after 12 layerings of dehydration treating tower phase splitter, upper materials dehydration treating tower reflux pump 13 is delivered to dehydration treating tower 8 trim the top of column, and lower floor's material is sent to wastewater trough and collects; Dehydration treating tower 8 tower reactor materials pump into n-butyl acetate finished product condenser 15 by n-butyl acetate discharge pump 14, cooling after, obtain ethyl acetate finished product.It is preferred technical scheme.
The production method of n-butyl acetate of the present invention, described dehydration treating tower 8 tower tops distillate gas and enter between recovery tower reboiler 17 pipes, after material-heat-exchanging in pipe, enter again supplementary heat exchanger 25, after the charging heat exchange of dehydration treating tower (8), need not be again through further cooling, the condensation of dehydration treating tower overhead condenser, and directly enter 12 layerings of dehydration treating tower phase splitter.Can save dehydration treating tower overhead condenser.
The production method of n-butyl acetate of the present invention, described dehydration treating tower 8 is board-like valve tray column, theoretical plate number is 52.
The production method of n-butyl acetate of the present invention, is characterized in that the operational condition of described dehydration treating tower 8 is as follows:
The production method of n-butyl acetate of the present invention, is characterized in that comprising following operation steps:
1. esterification
Raw material butanols and acetic acid react esterifying kettle 1 is interior, the n-butyl acetate and the water that generate, after vaporization, carry part material and enter esterification distillation tower 3, proceed esterification and through fractionation by distillation in esterification distillation tower 3, tower top distillates that the ternary azeotrope of n-butyl acetate, fourth alcohol and water is cooling through esterification condenser A4, esterification condenser B5, after condensation, enter esterification phase splitter 6, the thick ester in upper strata is through esterification reflux pump 7, and part pumps into esterification distillation tower 3, as trim the top of column; Another part pumps into dehydration treating tower 8;
2.. dehydration is refining
From the thick ester of esterification operating system, enter in dehydration treating tower 8, utilize dehydration treating tower 8 tower tops to distillate heat that gas the carries thermal source as recovery tower reboiler 17; Described tower top distillates gas and first enters between recovery tower reboiler 17 pipes, with material-heat-exchanging in pipe, self obtain simultaneously cooling, then through dehydration treating tower condenser A 10 further after cooling, condensation, enter phase splitter phase-splitting, organic phase material is all admitted to the 8 top total refluxs of dehydration treating tower; Lower floor's material is sent to recovery tower feed storage tank 18; Dehydration treating tower 8 tower reactor materials pump into n-butyl acetate finished product condenser 15 by n-butyl acetate discharge pump 14, cooling after, obtain ethyl acetate finished product;
3. reclaim
From the waste water of recovery tower feed storage tank 18, send into recovery tower 16 by reclaiming fresh feed pump 19, by the feed composition in Distillation recovery waste water and a small amount of product, recovery tower reboiler 17 is used to autospasy water treating tower 8 tower tops and distillates heat that gas carries as thermal source, recovery tower 16 overhead product material through recovery tower condenser A20 and recovery tower condenser B 21 condensations, enter recovery tower return tank 22, again by recovery tower reflux pump 23 by the extraction of partial condensation liquid, de-esterifying operating system, participates in reaction again; Waste water in recovery tower 16 tower reactors reaches after draining technology index, delivers to Sewage treatment systems.
The production method of n-butyl acetate of the present invention has following positively effect compared to existing technology:
1. provide that a kind of facility investment economizes, production cost is lower, reduced energy consumption, the production method of the n-butyl acetate of saving water resource.
2. same scale n-butyl acetate production equipment, the steam consumption in dehydration rectifying reduces 10%, and ton product can steam saving 0.2 ton, 100 meters of overhead condensation water saving per hour
3.
3. can reduce the facility investment of dehydration treating tower overhead condenser or save dehydration treating tower overhead condenser.
4. 40,000 tons/year are produced after n-butyl acetate plant modification in Linyi Golden Yimeng Biotechnology Co., Ltd. according to method of the present invention, during test is on probation, reduce production costs 40 yuan/ton, realize energy-saving and cost-reducing 1,840,000 yuan/year.
Accompanying drawing explanation
Fig. 1 is n-butyl acetate production equipment schematic flow sheet of the prior art.
Fig. 2 is a kind of n-butyl acetate production equipment schematic flow sheet of the inventive method.
Fig. 3 is a kind of preferred schematic flow sheet of n-butyl acetate production equipment of the inventive method.
In figure: 1-esterifying kettle 1, 2-esterification reboiler, 3-esterification distillation tower, 4-esterification condenser A, 5-esterification condenser B, 6-esterification phase splitter, 7-esterification reflux pump, the 8-treating tower that dewaters, 9-dehydration treating tower reboiler, 10-dehydration treating tower condenser A, 11-dehydration treating tower condenser B, 12-dehydration treating tower phase splitter, 13-dehydration treating tower reflux pump, 14-n-butyl acetate discharge pump, 15-n-butyl acetate finished product condenser, 16-recovery tower, 17-recovery tower reboiler, 18-recovery tower feed storage tank, 19-reclaims fresh feed pump, 20-recovery tower condenser A, 21-recovery tower condenser B, 22-recovery tower return tank, 23-recovery tower reflux pump, 24-connection line, 25-supplementary heat exchanger.
There is embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
The production method of n-butyl acetate of the present invention, comprises following operation steps:
1. esterification
Raw material butanols and acetic acid react esterifying kettle 1 is interior, the n-butyl acetate and the water that generate, after vaporization, carry part material and enter esterification distillation tower 3, proceed esterification and through fractionation by distillation in esterification distillation tower 3, tower top distillates that the ternary azeotrope of n-butyl acetate, fourth alcohol and water is cooling through esterification condenser A 4, esterification condenser B 5, after condensation, enter esterification phase splitter 6, the thick ester in upper strata is through esterification reflux pump 7, and part pumps into esterification distillation tower 3, as trim the top of column; Another part pumps into dehydration treating tower 8;
2.. dehydration is refining
From the thick ester of esterification operating system, enter in dehydration treating tower 8, utilize dehydration treating tower 8 tower tops to distillate heat that gas the carries thermal source as recovery tower reboiler 17; Described tower top distillates gas and first enters between recovery tower reboiler 17 pipes, with material-heat-exchanging in pipe, self obtain simultaneously cooling, then through dehydration treating tower condenser A 10 further after cooling, condensation, enter phase splitter phase-splitting, organic phase material is all admitted to the 8 top total refluxs of dehydration treating tower; Lower floor's material is sent to recovery tower feed storage tank 18; Dehydration treating tower 8 tower reactor materials pump into n-butyl acetate finished product condenser 15 by n-butyl acetate discharge pump 14, cooling after, obtain ethyl acetate finished product;
Described dehydration treating tower 8 is board-like valve tray column, and theoretical plate number is 52.
The operational condition of dehydration treating tower 8 is as follows:
3. reclaim
From the waste water of recovery tower feed storage tank 18, send into recovery tower 16 by reclaiming fresh feed pump 19, by the feed composition in Distillation recovery waste water and a small amount of product, recovery tower reboiler 17 is used to autospasy water treating tower 8 tower tops and distillates heat that gas carries as thermal source, recovery tower 16 overhead product material through recovery tower condenser A20 and recovery tower condenser B 21 condensations, enter recovery tower return tank 22, again by recovery tower reflux pump 23 by the extraction of partial condensation liquid, de-esterifying operating system, participates in reaction again; Waste water in recovery tower 16 tower reactors reaches after draining technology index, delivers to Sewage treatment systems.
Embodiment 2
According to the method for embodiment 1 and step, difference is:
1.. dehydration treating tower 8 tower tops distillate gas and enter between recovery tower reboiler 17 pipes, after material-heat-exchanging in pipe, enter again supplementary heat exchanger 25, charging heat exchange with dehydration treating tower 8, the liquid that condensation is got off enters dehydration treating tower condenser A (10, then enter after 12 layerings of dehydration treating tower phase splitter, upper materials dehydration treating tower reflux pump 13 is delivered to dehydration treating tower 8 trim the top of column, and lower floor's material is sent to wastewater trough and collects; Dehydration treating tower 8 tower reactor materials pump into n-butyl acetate finished product condenser 15 by n-butyl acetate discharge pump 14, cooling after, obtain ethyl acetate finished product.
2.. the operational condition of dehydration treating tower (8) is as follows:
Embodiment 3
According to the method for embodiment 1 and step, difference is:
1.. dehydration treating tower 8 tower tops distillate gas and enter between recovery tower reboiler 17 pipes, after material-heat-exchanging in pipe, enter again supplementary heat exchanger 25, with dehydration treating tower 8 charging heat exchange after, need not be again through further cooling, the condensation of dehydration treating tower overhead condenser, and directly enter 12 layerings of dehydration treating tower phase splitter.
2.. the operational condition of dehydration treating tower 8 is as follows:
Embodiment 4.
According to the method for embodiment 1 and step, difference is: the operational condition of dehydration treating tower 8 is as follows:
Claims (5)
1. a production method for n-butyl acetate, comprises esterification distillation procedure system, dehydration purification operations system and reclaims distillation procedure system, it is characterized in that comprising following operation steps:
1. esterification
Raw material butanols reacts in esterifying kettle (1) with acetic acid, the n-butyl acetate and the water that generate, after vaporization, carry part material and enter esterification distillation tower (3), in esterification distillation tower (3), proceed esterification and through fractionation by distillation, tower top distillates that the ternary azeotrope of n-butyl acetate, fourth alcohol and water is cooling through esterification condenser A (4), esterification condenser B (5), after condensation, enter esterification phase splitter (6), the thick ester in upper strata is through esterification reflux pump (7), part pumps into esterification distillation tower (3), as trim the top of column; Another part pumps into dehydration treating tower (8);
2.. dehydration is refining
From the thick ester of esterification operating system, enter in dehydration treating tower (8), utilize dehydration treating tower (8) tower top to distillate heat that gas the carries thermal source as recovery tower reboiler (17); Described tower top distillates gas and first enters between recovery tower reboiler (17) pipe, with material-heat-exchanging in pipe, self obtain cooling simultaneously, again through dehydration treating tower condenser A (10) further after cooling, condensation, enter phase splitter phase-splitting, organic phase material is all admitted to the top total reflux of dehydration treating tower (8); Lower floor's material is sent to recovery tower feed storage tank (18); Dehydration treating tower (8) tower reactor material pumps into n-butyl acetate finished product condenser (15) by n-butyl acetate discharge pump (14), cooling after, obtain ethyl acetate finished product; The operational condition of described dehydration treating tower (8) is as follows:
3. reclaim
From the waste water of recovery tower feed storage tank (18), send into recovery tower (16) by reclaiming fresh feed pump (19), by the feed composition in Distillation recovery waste water and a small amount of product, recovery tower reboiler (17) is used to autospasy water treating tower (8) tower top and distillates heat that gas carries as thermal source, recovery tower (16) overhead product material is through recovery tower condenser A (20) and recovery tower condenser B (21) condensation, enter recovery tower return tank (22), again by recovery tower reflux pump (23) by the extraction of partial condensation liquid, de-esterifying operating system, again participate in reaction, waste water in recovery tower (16) tower reactor reaches after draining technology index, delivers to Sewage treatment systems.
2. according to the production method of the n-butyl acetate of claim 1, it is characterized in that the working pressure >=0.3MPa of described dehydration purification operations system, described utilization dehydration treating tower (8) tower top distillates heat that gas the carries thermal source as recovery tower reboiler (17), to substitute the needed heating steam of recovery tower reboiler (17) completely, need not other supplemental heat source.
3. according to the production method of the n-butyl acetate of claim 1, treating tower (8) tower top that it is characterized in that dewatering distillates gas and enters between recovery tower reboiler (17) pipe, after material-heat-exchanging in pipe, enter again supplementary heat exchanger (25), with the charging heat exchange of dehydration treating tower (8), the liquid that condensation is got off enters dehydration treating tower condenser A (10), then enter after the layering of dehydration treating tower phase splitter (12), upper materials dehydration treating tower reflux pump (13) is delivered to dehydration treating tower (8) trim the top of column, lower floor's material is sent to wastewater trough and collects, dehydration treating tower (8) tower reactor material pumps into n-butyl acetate finished product condenser (15) by n-butyl acetate discharge pump (14), cooling after, obtain n-butyl acetate finished product.
4. according to the production method of the n-butyl acetate of claim 1, it is characterized in that described dehydration treating tower (8) tower top distillates gas and enters between recovery tower reboiler (17) pipe, after material-heat-exchanging in pipe, enter again supplementary heat exchanger (25), after the charging heat exchange of dehydration treating tower (8), need not be again through further cooling, the condensation of dehydration treating tower overhead condenser, and directly enter the layering of dehydration treating tower phase splitter (12).
5. according to the production method of the n-butyl acetate of claim 1, it is characterized in that described dehydration treating tower (8) is board-like valve tray column, theoretical plate number is 52.
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| CN103254068A (en) * | 2013-05-22 | 2013-08-21 | 江门天诚溶剂制品有限公司 | Energy-saving multi-effect distillation process for producing n-butyl acetate |
| CN103724192B (en) * | 2013-09-05 | 2015-09-23 | 百川化工(如皋)有限公司 | A kind of method of energy-saving purified acetic acid ester |
| CN104513159A (en) * | 2014-11-28 | 2015-04-15 | 江门天诚溶剂制品有限公司 | Butyl acetate energy saving production method |
| CN105585486A (en) * | 2016-02-19 | 2016-05-18 | 邢台市茂新化工产品有限公司 | Process for extracting and deacidifying n-butyl acetate coarse ester |
| CN110935186A (en) * | 2019-11-12 | 2020-03-31 | 临沂市金沂蒙生物科技有限公司 | Novel heat coupling rectification process in acetate production process |
| CN110862321A (en) * | 2019-11-12 | 2020-03-06 | 临沂市金沂蒙生物科技有限公司 | New process for combined rectification of ethyl acetate and n-butyl acetate |
| CN113292429B (en) * | 2021-05-10 | 2022-10-28 | 浙江建业化工股份有限公司 | Production system and production method of isobutyl acetate for high-end paint |
| CN114751822B (en) * | 2022-03-16 | 2024-04-09 | 浙江建业化工股份有限公司 | Device for producing n-propyl acetate by thermal coupling and production method thereof |
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| US20050107629A1 (en) * | 2003-11-17 | 2005-05-19 | Hershberger Brian L. | Method for producing ethyl acrylate |
| CN100503549C (en) * | 2007-06-22 | 2009-06-24 | 张立省 | Method for reusing waste water reclaimed from ethyl acetate production |
| CN101830799B (en) * | 2010-05-25 | 2013-05-08 | 临沂市金沂蒙生物科技有限公司 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
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Denomination of invention: Production method of n-butyl acetate Effective date of registration: 20211129 Granted publication date: 20140521 Pledgee: Linshu sub branch of Linshang Bank Co.,Ltd. Pledgor: LINYI JINYIMENG BIOTECHNOLOGY CO.,LTD. Registration number: Y2021980013410 |